HRID1020805
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 2,5,6-trichloronicotinonitrile (30 g, 144.92 mmol, 1.00 equiv) in sulfuric acid (98%, 162 mL, 1.00 equiv) was stirred for 1 h at 60° C. in an oil bath. The reaction mixture was cooled and then quenched by the addition of water/ice. The solid was collected by filtration and dried in an oven under reduced pressure. This resulted in 26 g of 2,5,6-trichloronicotinamide as a white solid. LC-MS (ES, m/z): 225 [M+H]+. 1H-NMR (300 MHz, DMSO-d6) δ (ppm) 9.38 (1H, s), 8.12 (1H, s), 7.95 (1H, s).
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- customquenched by the addition of water/ice
- filtrationThe solid was collected by filtration
- customdried in an oven under reduced pressure
- customThis resulted in 26 g of 2,5,6-trichloronicotinamide as a white solid